Skip to content

JASCO JASCO

  • News
  • Events
  • E-Store
  • My Account
  • Contact Us
  • Worldwide
Search
Click to view menu
MENUMENU
  • Products
    • Chromatography
      • HPLC
      • RHPLC
      • UHPLC
      • LC-MS
      • Preparative LC
      • Analytical SFC
      • Semi-Preparative SFC
      • Hybrid SFC
      • Fuel Analysis by SFC-FID
      • Preparative SFC
      • Supercritical Fluid Extraction
      • Chromatography Software
    • Molecular Spectroscopy
      • Circular Dichroism
      • High-Throughput CD
      • Vibrational CD
      • Circularly Polarized Luminescence (CPL)
      • Polarimeters
      • FTIR Spectrometers
      • FTIR Microscopy
      • FTIR Portable
      • Raman Microscopy
      • Palmtop Raman Spectrometer
      • Probe Raman
      • UV-Visible/NIR Spectrophotometers
      • UV-Visible/NIR Microscopy
      • Fluorescence Spectrophotometers
      • Film Thickness
      • Spectra Manager™ Suite
    • Refurbished
      • Refurbished HPLC Systems
      • HPLC Switching Valves
      • FTIR Accessories
  • Service
    • Service and Support Plans
    • Service Request Form
  • Applications
  • KnowledgeBase
  • Learning Center
    • Best Practice
      • Circular Dichroism Tips & Tricks for Biological Samples
      • CD Scale Calibration with ACS
      • Fluorescence Tips & Tricks
      • Raman Spectroscopy Tips & Tricks
    • Training Videos
      • ChromNAV
      • SF-NAV
      • Circular Dichroism
      • UV-Visible/NIR
      • Fluorescence
    • Training Seminars
      • Training Registration Form
    • Webinars
    • eBooks
    • Theory
      • Theory of Molecular Spectroscopy
      • Chromatography
  • About Us
    • President’s Message
    • Contact
    • History
    • Careers
  • News
  • Events
  • Worldwide
  • Shop
  • My Account
  • Contact Us

Home / Applications / Analysis of Pesticides using Supercritical Fluid Chromatography with Mass Spectrometry (SFC-MS)

  • Industry

  • Technique

Analysis of Pesticides using Supercritical Fluid Chromatography with Mass Spectrometry (SFC-MS)

By Heather Haffner

PDF IconDownload This Application

August 19, 2022

Introduction

Pesticide analysis is required for consumer safety for food consumption. In 1996 the US FDA implemented regular monitoring of domestic and imported foods. There are 1000 registered pesticides by the US and 1100 by the European Union. The upper allowable limit is 10ppb or less. Japan has 16 pesticides that have zero tolerance. With the above requirements, extremely sensitive pesticide analysis is required.

HPLC with fluorescence detection is a common system used to analyze certain pesticides. Fluorescence is a very sensitive detector, but of course it does not aid in the identification that MS can offer. The speed of SFC combined with the sensitivity and identification of Mass Spectrometry was explored for pesticides.

Jasco PU-2080 Plus pump

Experimental

Figure 1. Structures of the 6 pesticides used for initial UV detector testing.
Figure 2. Overlay of SFC-UV chromatograms of 6 Pesticides. 1. Malathion, 2. Chloryriphos, 3. Carbofuran, Coumaphos, 5. Carbaryl, 6. Duron.
Figure 3. Stacked SFC-UV chromatograms of Carbaryl.

The structures of the 6 pesticides is shown in figure 1 and those 6 were each run and an overlay of their chromatograms is shown in figure 2. Carbaryl is shown at various concentrations in figure 3. Five out of the six pesticides were detected at 1ppm with UV alone. The MS was next used to increase the sensitivity.

Figure 4. SFC-MS SIM chromatogram of 6 pesticide mix (0.5ppm each).Column SFCpak Sil-5 (4.6 x 250mm, 5um)

The SFC-MS chromatogram of the 6 pesticides at 0.5ppm and the corresponding spectra are shown in figure 4 and 5, respectively. The sensitivity was test at various concentrations 0.5pmm to 2ppb (Figure 6). A mixture of 32 pesticides (each 0.5ppm) was injected and 26 of them were detected and identified using the same conditions on the silica column. The identities and the retention times of each are shown in table 1.

Figure 5. MS Peak Spectra Confirming Pesticide Identity.
Figure 6. Stacked SFC-MS SIM chromatograms of 6 pesticide mix. Conditions were the same as shown in previous slides. S/N of 2 or greater for all 6 pesticides at 2ppb.
Figure 7. Overlay of XIC of 26 pesticides using SFC-MS.26 of 32 pesticides were detected using SFC-MS.

Table 1. List of pesticides from figure 7 and their retention times.

Conclusion

The SFC-UV detected 5 out of 6 pesticides at 1ppm. All 6 pesticides produced a S/N of greater than 2 at 2ppb on a single quad MS in just over 5 minutes using SFC-MS. The SFC-MS identified 26 out of 32 pesticides in 6 minutes.

This document has been prepared based on information available at the time of publication and is subject to revision without notice. Although the contents are checked with the utmost care, we do not guarantee their accuracy or completeness. JASCO Corporation assumes no responsibility or liability for any loss or damage incurred as a result of the use of any information contained in this document. Copyright and other intellectual property rights in this document remain the property of JASCO Corporation. Please do not attempt to copy, modify, redistribute, or sell etc. in whole or in part without prior written permission.

Featured Products:

  • Tandem LC-MS

  • Single Quadrupole LC-MS

  • SFC-4000 Analytical SFC for routine separation to method development.

    Analytical SFC System

About the Author

JASCO Application Note

Analysis of Pesticides using Supercritical Fluid Chromatography with Mass Spectrometry (SFC-MS)

Introduction

Pesticide analysis is required for consumer safety for food consumption. In 1996 the US FDA implemented regular monitoring of domestic and imported foods. There are 1000 registered pesticides by the US and 1100 by the European Union. The upper allowable limit is 10ppb or less. Japan has 16 pesticides that have zero tolerance. With the above requirements, extremely sensitive pesticide analysis is required.

HPLC with fluorescence detection is a common system used to analyze certain pesticides. Fluorescence is a very sensitive detector, but of course it does not aid in the identification that MS can offer. The speed of SFC combined with the sensitivity and identification of Mass Spectrometry was explored for pesticides.

Jasco PU-2080 Plus pump

Experimental

Figure 1. Structures of the 6 pesticides used for initial UV detector testing.
Figure 2. Overlay of SFC-UV chromatograms of 6 Pesticides. 1. Malathion, 2. Chloryriphos, 3. Carbofuran, Coumaphos, 5. Carbaryl, 6. Duron.
Figure 3. Stacked SFC-UV chromatograms of Carbaryl.

The structures of the 6 pesticides is shown in figure 1 and those 6 were each run and an overlay of their chromatograms is shown in figure 2. Carbaryl is shown at various concentrations in figure 3. Five out of the six pesticides were detected at 1ppm with UV alone. The MS was next used to increase the sensitivity.

Figure 4. SFC-MS SIM chromatogram of 6 pesticide mix (0.5ppm each).Column SFCpak Sil-5 (4.6 x 250mm, 5um)

The SFC-MS chromatogram of the 6 pesticides at 0.5ppm and the corresponding spectra are shown in figure 4 and 5, respectively. The sensitivity was test at various concentrations 0.5pmm to 2ppb (Figure 6). A mixture of 32 pesticides (each 0.5ppm) was injected and 26 of them were detected and identified using the same conditions on the silica column. The identities and the retention times of each are shown in table 1.

Figure 5. MS Peak Spectra Confirming Pesticide Identity.
Figure 6. Stacked SFC-MS SIM chromatograms of 6 pesticide mix. Conditions were the same as shown in previous slides. S/N of 2 or greater for all 6 pesticides at 2ppb.
Figure 7. Overlay of XIC of 26 pesticides using SFC-MS.26 of 32 pesticides were detected using SFC-MS.

Table 1. List of pesticides from figure 7 and their retention times.

Conclusion

The SFC-UV detected 5 out of 6 pesticides at 1ppm. All 6 pesticides produced a S/N of greater than 2 at 2ppb on a single quad MS in just over 5 minutes using SFC-MS. The SFC-MS identified 26 out of 32 pesticides in 6 minutes.

This document has been prepared based on information available at the time of publication and is subject to revision without notice. Although the contents are checked with the utmost care, we do not guarantee their accuracy or completeness. JASCO Corporation assumes no responsibility or liability for any loss or damage incurred as a result of the use of any information contained in this document. Copyright and other intellectual property rights in this document remain the property of JASCO Corporation. Please do not attempt to copy, modify, redistribute, or sell etc. in whole or in part without prior written permission.
28600 Mary’s Court, Easton, MD 21601 USA • (800) 333-5272 • Fax: (410) 822-7526 • jascoinc.com/applications

Close

Designed in Tokyo. TRUSTED globally.

View our support plans

Connect with JASCO

  • Facebook
  • Twitter
  • LinkedIn
  • JASCO Sales
  • 800-333-5272

Receive the latest promotions and special offers

  • This field is for validation purposes and should be left unchanged.
  • Careers
  • Press Kit
  • JASCO Privacy Policy
  • Sitemap
  • Environmental Policy

© , JASCO. All Rights Reserved.